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Crystal structures of diphosphinated group 6 Fischer alkoxy carbenes

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Abstract

The crystal structures of four diphosphinated Group 6 Fischer alkoxy carbenes with the compositions fac-(dppe)(CO)3M–C(OR′)(R) (R = Me, R′ = Et, M = Cr, 1; R = Ph, R′ = Me, M = Cr, 2; R = Me, R′ = Me, M = W, 3; R/OR′ = 3-methyl-2-oxacyclopentylidenyl, M = Cr, 4) have been determined at 243 K. Compound 1 crystallizes in the monoclinic system, space group P21/c with a = 11.2243(11) Å, b = 18.5998(18) Å, c = 15.1260(15) Å, β = 107.056(4), V = 3019.0(5) Å3, and Z = 4. Compound 2 crystallizes in the monoclinic system, space group P21/c with a = 11.8102(9) Å, b = 18.3152(14) Å, c = 15.0262(12) Å, β = 93.753(3), V = 3243.3(4) Å3, and Z = 4. Compound 3 crystallizes in the monoclinic system, space group P21/c with a = 11.3458(6) Å, b = 18.5772(9) Å, c = 15.3883(8) Å, β = 108.576(6), V = 3074.5(3) Å3, and Z = 4. Compound 4 crystallizes in the orthorhombic system, space group Pna21 with a = 22.6509(14) Å, b = 9.8118(6) Å, c = 13.7507(8) Å, V = 3056.0(3) Å3, and Z = 4. Steric repulsions with the dppe ligand favor a conformation with the alkoxy moiety directed toward the dppe backbone, in an E geometry, in 1–4.

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References

  1. Mills, O.S.; Redhouse, A.D. Chem. Commun. 1966, 814–815.

  2. Xu, Y.-C.; Wulff, W.D. J. Org. Chem. 1987, 52, 3263–3275.

    Google Scholar 

  3. Wulff, W.D.; Anderson, B.A.; Toole, A.J.; Xu, Y.-C. Inorg. Chim. Acta 1994, 220, 215–231.

    Google Scholar 

  4. Hsung, R.P.; Xu, Y.-C.; Wulff, W.D. Tetrahedron Lett. 1995, 36, 8159–8162.

    Google Scholar 

  5. Hegedus, L.S.; Schultze, L.M.; Toro, J.; Yijun, C. Tetrahedron 1985, 41, 5833–5838.

    Google Scholar 

  6. Herndon, J.W.; Zora, M. Synlett. 1993, 363–364.

  7. Cooke, M.D.; Fischer, E.O. J. Organomet. Chem. 1973, 56, 279–284.

    Google Scholar 

  8. Park, Y.-I.; Kim S.-J.; Ko, J.-J.; Kang, S.O. Bull. Korean Chem. Soc. 1997, 18, 1061–1066.

    Google Scholar 

  9. Arrieta, A.; Cossío, F.P.; Fernández, I.A.; Gómez-Gallego, M.; Lecea, B.; Mancheño, M.J.; Sierra, M.A. J. Am. Chem. Soc. 2000, 122, 11509–11510.

    Google Scholar 

  10. Tisserat, C.G. Masters Thesis, California State Polytechnic University, Pomona, 2000.

  11. Fischer, E.O.; Maasböl, A. J. Organomet. Chem. 1968, 12, P15–P17

    Google Scholar 

  12. Werner, H.; Rascher, H. Inorg. Chim. Acta 1968, 2, 181–185

    Google Scholar 

  13. Fischer, E.O.; Maasböl, A. Angew. Chem., Int. Ed. Engl. 1964, 3, 580–581.

    Google Scholar 

  14. Aumann, R.; Fischer, E.O. Angew. Chem. Int. Ed. Engl. 1967, 6, 879–880.

    Google Scholar 

  15. SMART, Software for the CCD Detector System, version 5.050 (NT); Bruker Analytical X-ray Systems: Madison, WI, 1998.

  16. SAINT, Software for the CCD Detector System, version 5.01 (NT); Bruker Analytical X-ray Systems: Madison, WI, 1998.

  17. Blessing, R. H. SADABS, Program for Absorption Corrections Using Siemens CCD Based on the Method of Robert Blessing: Acta Crystallogr. 1995, A51, 33–38.

    Google Scholar 

  18. Sheldrick, G.M. SHELXS-90, Program for the Solution of Crystal Structure; University of Göttingen: Germany, 1990.

    Google Scholar 

  19. Sheldrick, G.M. SHELXL-97, Program for the Refinement of Crystal Structure; University of Göttingen: Germany, 1997.

    Google Scholar 

  20. SHELXTL 5.10, Program Library for Structure Solution and Molecular Graphics, PC Version; Bruker Analytical X-ray Systems: Madison, WI, 1998.

  21. Farrugia, L.J. J. Appl. Crystallogr. 1997, 30, 565.

    Google Scholar 

  22. Morton, D.A.V.; Orpen, A.G. J. Chem. Soc., Dalton Trans. 1992, 641–653.

  23. Arndtsen, B.A.; Schoch, T.K.; McElwee-White, L. J. Am. Chem. Soc. 1992, 114, 7041–7047.

    Google Scholar 

  24. Kreiter, C.G.; Fischer, E.O. Angew. Chem., Int. Ed. Engl. 1969, 8, 761–762.

    Google Scholar 

  25. Schubert, U. Coord. Chem. Rev. 1984, 261–286.

  26. Wang, C.-C.; Wang, Y.; Liu, H.-J.; Lin, K.-J.; Chou, L.-K.; Chan, K.-S. J. Phys. Chem. A 1997, 101, 8887–8901.

    Google Scholar 

  27. Huttner, G.; Lorenz, H. Chem. Ber. 1975, 108, 1864–1870.

    Google Scholar 

  28. Dötz, K.H.; Kuhn, W.; Ackermann, K.Z. Naturforsch. B 1983, 38, 1351–1356.

    Google Scholar 

  29. Krüger, C; Goddard, R.; Claus, K.H. Z. Naturforsch. B 1983, 38, 1431–1440.

    Google Scholar 

  30. Dötz, K.H.; Kuhn, W.; Thewalt, U. Chem. Ber. 1985, 118, 1126–1132.

    Google Scholar 

  31. Aumann, R.; Hinterding, P.; Krüger, C.; Betz, P. Chem. Ber. 1990, 123, 1847–1852.

    Google Scholar 

  32. Lu, T. Masters Thesis, California State Polytechnic University, Pomona, 2002.

  33. Beddoes, R.L.; Grime, R.W.; Hussain, Z.I.; Whiteley, M.W. J. Organomet. Chem. 1996, 526, 371–378.

    Google Scholar 

  34. Anglin, J.R.; Calhoun, H.P.; Graham, W.A.G. Inorg. Chem. 1977, 16, 2281–2288.

    Google Scholar 

  35. Reinheimer, E.W. Masters Thesis, California State Polytechnic University, Pomona, 2002.

  36. Perry, W.B.; Schaaf, T.F.; Jolly, W.L.; Todd, L.J.; Cronin, D.L. Inorg. Chem. 1974, 13, 2038–2039. (see also Ref. 19).

    Google Scholar 

  37. Mills, O.S.; Redhouse, A.D. J. Chem. Soc. A 1968, 642–647.

  38. Dötz, K.H. Angew. Chem. Int. Ed. Engl. 1984, 23, 587–606.

    Google Scholar 

  39. Fischer, E.O.; Aumann, R. Chem. Ber. 1969, 102, 1495–1503.

    Google Scholar 

  40. Guy, M.P.; Guy, J.T. Jr.; Bennett, D.W. Organometallics 1986, 5, 1696–1702.

    Google Scholar 

  41. Alvarez, C.; Pacreau, A.; Parlier, A.; Rudler, H. Organometallics 1987, 6, 1057–1064.

    Google Scholar 

  42. Macomber, D.W.; Hung, M.-H.; Verma, A.G. Organometallics 1988, 7, 2072–2074.

    Google Scholar 

  43. Casey, S.P.; Anderson, R.L. J. Org. Chem. 1974, 73, C28–C30.

    Google Scholar 

  44. Lattuada, L.; Licandro, E.; Maiorana, S.; Molinari, H.; Papagni, A. Organometallics 1991, 10, 807–812.

    Google Scholar 

  45. Careri, M.; Mangia, A.; Manini, P.; Predieri, G.; Licandro, E.; Papagni, A. J. Chromatogr. A 1996, 730, 231–240.

    Google Scholar 

  46. Weyershausen, B.; Nieger, M.; Dötz, K.H. Organometallics, 1998, 17, 1602–1607.

    Google Scholar 

  47. Bianchini, C.; Marchi, A.; Mantovani, N.; Marvelli, L.; Masi, D.; Peruzzini, M.; Rossi, R. Eur. J. Inorg. Chem. 1998, 211–219.

  48. Beddoes, R.L.; Grime, R.W.; Hussain, Z.I.; Whiteley, M.W. J. Chem. Soc., Dalton. Trans. 1996, 3893–3895.

  49. O'Connor, J.M.; Pu, L.; Rheingold, A.L. J. Am. Chem. Soc. 1990, 112, 6232–6247.

    Google Scholar 

  50. Adams, H.; Bailey, N.A.; Grayson, M.; Ridgway, C.; Smith, A.J.; Taylor, P.; Winter, M.J. Organometallics, 1990, 9, 2621–628.

    Google Scholar 

  51. Huheey, J.E.; Keiter, E.A.; Keiter, R.L. Inorganic Chemistry; HarperCollins: New York, 1993; pp 425–431.

    Google Scholar 

  52. Derensbourg, M. Y.; Darensbourg, D. J. Inorg. Chem. 1970, 9, 32–39.

    Google Scholar 

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Correspondence to Joe A. Casalnuovo.

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Reinheimer, E.W., Kantardjieff, K.A., Herron, S.R. et al. Crystal structures of diphosphinated group 6 Fischer alkoxy carbenes. Journal of Chemical Crystallography 33, 503–514 (2003). https://doi.org/10.1023/A:1024258904251

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